関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 反応物 | (22E)-5,7,22-Ergostatriene-1alpha,3beta,25-triol | HCID 67831887 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1alpha,25-Dihydroxyvitamin D2 | HCID 9547243 | 22.3% |
反応手順
(22E)-5,7,22-Ergostatriene-1α,3β,25-triol (Ia) (100 mg, 0.23 mmol) was dissolved in a mixed solution of ether (950 ml) and tetrahydrofuran (50 ml), and the solution was irradiated with high pressure mercury lamp using an 1.5% aqueous potassium nitrate solution as a filter with water cooling in a nitrogen stream for 3 minutes. From the reaction solution was distilled off the solvent and the residue containing previtamin D was dissolved in ethanol (30 ml) and the solution was refluxed for one hour. After distilling off ethanol, the residue was purified by high pressure liquid chromatography (HPLC) (column: LiChrosorb® Si60 (7 μm), φ25×250 mm, Merck Co., Ltd.; column effluent: 4% methanol-methylene chloride; flow rate: 8.0 ml/min; detected at 264 nm) to give 22 mg of the title compound (IIa) which was recrystallized from hexane-ether. m.p. 168°-170° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05087709 |
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| 出典データセット | uspto-grants-1992_02 |
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| ORD ID | ord-5de84c49686b41e5a8f0c39605e3a2fd |
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| 出典メモ | uspto-grants-1992_02 |
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